CN118243591A - Porosity testing method and device for irregularly-shaped rock core - Google Patents
Porosity testing method and device for irregularly-shaped rock core Download PDFInfo
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- 238000012360 testing method Methods 0.000 title claims abstract description 117
- 239000011435 rock Substances 0.000 title abstract description 31
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- 238000005481 NMR spectroscopy Methods 0.000 claims abstract description 197
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 146
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 141
- 239000001257 hydrogen Substances 0.000 claims abstract description 141
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- 239000003550 marker Substances 0.000 claims description 17
- 238000007789 sealing Methods 0.000 claims description 14
- 230000035945 sensitivity Effects 0.000 claims description 10
- 229910000365 copper sulfate Inorganic materials 0.000 claims description 6
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 6
- 238000000685 Carr-Purcell-Meiboom-Gill pulse sequence Methods 0.000 claims description 4
- 238000005553 drilling Methods 0.000 abstract description 27
- 238000005520 cutting process Methods 0.000 abstract description 14
- 239000000523 sample Substances 0.000 description 302
- 238000005259 measurement Methods 0.000 description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 21
- 238000001035 drying Methods 0.000 description 14
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 10
- 239000004810 polytetrafluoroethylene Substances 0.000 description 10
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- 238000002360 preparation method Methods 0.000 description 9
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- 238000001514 detection method Methods 0.000 description 6
- 239000003921 oil Substances 0.000 description 6
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- 229930195733 hydrocarbon Natural products 0.000 description 4
- 150000002430 hydrocarbons Chemical class 0.000 description 4
- 238000005070 sampling Methods 0.000 description 4
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- 238000001225 nuclear magnetic resonance method Methods 0.000 description 3
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- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 2
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- 238000002459 porosimetry Methods 0.000 description 2
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- 238000004293 19F NMR spectroscopy Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials
- G01N15/088—Investigating volume, surface area, size or distribution of pores; Porosimetry
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N24/00—Investigating or analyzing materials by the use of nuclear magnetic resonance, electron paramagnetic resonance or other spin effects
- G01N24/08—Investigating or analyzing materials by the use of nuclear magnetic resonance, electron paramagnetic resonance or other spin effects by using nuclear magnetic resonance
- G01N24/081—Making measurements of geologic samples, e.g. measurements of moisture, pH, porosity, permeability, tortuosity or viscosity
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Abstract
The embodiment of the invention discloses a porosity testing method and device for an irregularly-shaped rock core, wherein the device comprises the following steps: the device comprises a magnet unit, a radio frequency unit, a spectrometer unit, a calculation unit and a sample tube; the magnet unit comprises a magnet which is used for providing a magnetic field for the volume scale standard sample, the hydrogen-containing liquid and the sample to be tested, and the magnetic field strength of the magnet is 0.1-0.2T; the radio frequency unit is used for detecting nuclear magnetic resonance signals of the volume calibration standard sample, the hydrogen-containing liquid and the sample to be detected, and comprises a radio frequency coil, wherein the radio frequency coil is provided with a nuclear magnetic resonance signal linear region, a nuclear magnetic resonance signal nonlinear region and a highest nuclear magnetic resonance signal region; the spectrometer unit is used for controlling the radio frequency unit to collect nuclear magnetic resonance signals of the volume calibration standard sample, the hydrogen-containing liquid and the sample to be detected; the calculating unit is used for calculating the porosity of the sample to be measured. According to the embodiment of the invention, the on-site rapid and high-precision testing of the porosity of the irregular-shaped core such as the sidewall coring core and the drilling cuttings by the drilling fluid can be realized.
Description
Technical Field
The application relates to the field of quick detection of geological samples in oilfield exploration sites, in particular to a porosity testing method and device for an irregularly-shaped rock core.
Background
The sidewall coring core and the drilling cuttings are rock specimens which are taken out of a target stratum during oil and gas exploration and reflect stratum conditions. The geological worker can clearly distinguish stratum evolution marks by researching analysis specimens, and important information of the stratum geological environment, sediment and structural characteristics, resource storage conditions and the like concerning oil gas development effects can be researched. The porosity, permeability and oil saturation of the sidewall coring core and the drilling cuttings are core indexes for evaluating oil and gas reserves and productivity, wherein the porosity is a primary index for reflecting reservoir space of a reservoir, so that the on-site rapid measurement of the porosity of the sidewall coring core and the drilling cuttings is an important content of logging service of an oilfield drilling site.
The sidewall coring core and drilling cuttings are irregularly shaped cores, and the earliest method of porosity testing was the drying method. The specific process for testing the porosity by adopting a drying method comprises the following steps: after the fresh sample is wiped with surface fluid (the pore is in a state of 100% saturated fluid, and the pore fluid is not exposed for a long time), the wet weight m 1 is firstly called, the fresh sample is baked in an oven at a high temperature until the mass is unchanged, the dry weight m 2 is called, and the porosity of the sample to be measured is:
，
in the formula For the porosity of the sample to be measured, m 1 is the wet weight of the sample, and the unit is g; m 2 is the dry weight of the sample, in g; /(I)The unit of the skeleton density is g/cm 3.
The problems with the drying process are: (1) Ignoring the density difference of oil and water in the pores, and approximating the density of the pore fluid by the density of water; (2) The skeleton density of the complex lithology is not easy to obtain, and an error is introduced by substituting an empirical value; (3) If crude oil with medium-high viscosity exists in the pore fluid, the drying method cannot thoroughly dry the sample, so that a dry weight measurement value is larger, and a measurement error is caused; (4) The sample is dried for a long time, the testing efficiency is low, and the hydrocarbon component in the sample is dried to cause environmental pollution (the drilling site is not usually provided with a fume hood for construction), so that the sample is harmful to the body of a tester.
With the popularization of laboratory Nuclear Magnetic Resonance (NMR) core measurement methods and instruments in the logging industry, NMR is applied to porosity detection of borehole wall coring cores and drill cuttings at the drilling site. In the prior art, the specific steps for testing the porosity of the sidewall coring core and the drilling cuttings by using the nuclear magnetic resonance method are as follows
The first step: and (3) wiping fresh sidewall coring core or drilling cuttings with wet filter paper, loading the surface fluid into a nuclear magnetic resonance test sample tube, setting reasonable measurement parameters, collecting nuclear magnetic resonance signals, and calculating by using nuclear magnetic resonance signal-volume scale values to obtain the pore volume V por of the sample to be measured.
And a second step of: and testing the skeleton volume V T of the sample to be tested by using a density balance.
The porosity of the sample to be measured is as follows:
，
In the middle of Porosity in units of; v por is the pore volume of the sample to be measured, the unit cm 3;VT is the skeleton volume of the sample to be measured, and the unit cm 3.
Compared with the traditional drying method, the nuclear magnetic resonance-density balance method solves the problems of hydrocarbon drying pollution and the like, and the precision of measuring the skeleton volume of the sample to be measured (namely, the total volume of the sample is equal to the pore volume and the skeleton volume) by the density balance also meets the requirements. However, the nuclear magnetic resonance-density balance method has obvious defects, firstly, the operation of testing the skeleton volume of a sample by the density balance method is complex, the test efficiency is low due to the fact that the sample is transferred twice, and if the sample has poor cementing property or cracks and the like, the situation of falling blocks or particles is caused during transfer, the measurement error with larger skeleton volume is caused; secondly, the practicality of the density balance method is poor and the human error is relatively large for the rock debris sample which is small particles. Therefore, although the nuclear magnetic resonance-density balance solves the problem of accurate measurement of the pore volume of a part of samples to be measured, the testing process is complex, the testing efficiency is low, and the typical problem of block samples which are unsuitable for rock fragments and easily broken and blocked is also existed, but the well wall coring of the drilling site generally only can core at a key layer due to high cost, and the rock fragments are a great number of geological samples which are produced by drilling construction cost and are extremely easy to obtain, and are the geological samples which are most expected to be accurately tested in the rock fragment logging of the drilling site.
In order to solve the problems of complicated sample transferring operation, large human error and the like in the nuclear magnetic resonance-density balance method, the method （[1]Dick M J, Green D, Kenney T, et al. Quick and simple porosity measurement at the well site[C]//International Symposium of the Society of Core Analysts. Vienna, Austria. 2017: 1-10.）, for simultaneously measuring the pore volume and the skeleton volume by using an NMR method is provided by Dick et al [1] in 2017, and the measuring method comprises the following steps:
1) The preparation stage: marking a fixed liquid adding liquid level line in the nuclear magnetic resonance signal linear region range of the sample tube, measuring a water volume V 1 when water is added to the liquid level line by a weighing method, measuring a nuclear magnetic resonance signal S 1 at the moment, and further obtaining a scale factor of the water volume and the nuclear magnetic resonance signal: k H= V1/ S1, wherein K H is a scale factor of water volume and nuclear magnetic resonance signal, cm 3;V1 is water volume when the liquid is added to the marked fixed liquid level line in the sample tube, cm 3;S1 is nuclear magnetic resonance signal when the liquid is added correspondingly, and the unit is dimensionless.
2) Test of sample to be tested step 1: after wiping fluid on the surface of fresh rock debris or rock core by wet filter paper, filling the fluid into a sample tube (and filling height is lower than liquid level line marked in the preparation stage), and testing nuclear magnetic resonance signals S 2 to obtain pore volume of a sample to be tested, wherein a calculation formula is as follows: wherein V por is the pore volume of the sample to be measured, cm 3;S2 is the NMR signal measured by the sample to be measured, and the unit is dimensionless.
3) Step 2, testing a sample to be tested: on the basis of step 1, the sample to be detected is not transferred, water is directly added into the sample tube to the liquid level line marked in the preparation stage, the liquid level line is overlapped with the liquid level line as much as possible, the nuclear magnetic resonance signal S 3.S3<S1 is measured, the signal difference between the liquid level line and the liquid level line is a sample skeleton which does not contribute to the H nuclear NMR signal, and therefore, the calculation formula of the volume of the sample skeleton is as follows: Wherein V G is the skeleton volume of the sample to be measured, cm 3;S3 is the nuclear magnetic resonance signal measured after the sample to be measured is added with water in the sample tube, and the unit is dimensionless.
Apparent volume=skeleton volume+pore volume of the sample to be measured, so the calculation formula of the porosity of the sample to be measured is:
。
according to the method, the liquid filling level line is kept the same as that of the sample to be tested in the preparation stage, the sample filling height of the sample to be tested is lower than that of the liquid filling level line, the porosity of the sample to be tested is calculated directly by combining nuclear magnetic resonance signal quantities in three states, and the water volume and the scale coefficient of the nuclear magnetic resonance signal are not needed to participate in calculation. Therefore, the NMR-H probe rock debris porosity measurement method has the advantages of simple method, simple operation, no need of transferring samples in the middle test process and the like. However, this method still has two disadvantages: (1) Human errors of the concave liquid level when the sample tube is filled lead to limited measurement accuracy of the skeleton volume; (2) In the step of testing the pore volume, the surface fluid wiping and cleaning residues of the fresh sample can cause the pore volume measurement value to be larger due to the surface tension effect, and further cause the porosity measurement value to be larger.
Aiming at factors such as difficult operation, personal errors, influence of residual fluid on the particle surface on results and the like of a fixed liquid level surface of an NMR-H probe rock debris porosimetry, fellah, mitchell [2-3] and the like of the Schlenmez company, the NMR-H, F probe rock debris porosimetry （[2]Fellah K, Utsuzawa S, Song Y Q, et al. Porosity of drill-cuttings using multinuclear 19F and 1H NMR measurements[J]. Energy&fuels, 2018, 32(7): 7467-7470.[3]Mitchell J, Valori A, Fordham E J. A robust nuclear magnetic resonance workflow for quantitative determination of petrophysical properties from drill cuttings[J]. Journal of Petroleum Science and Engineering, 2019, 174: 351-361.）, is proposed in 2018 and 2019, and the method comprises the following steps of:
1) Step 1 of the preparation stage: for the H probe, measuring the water volume V H1 of the water by a weighing method in the linear region of the nuclear magnetic resonance signal of the sample tube, and measuring the nuclear magnetic resonance signal S H1 at the moment, so as to obtain the scale coefficient of the water volume and the NMR signal: k H= VH1/ SH1, wherein K H is a scale factor of water volume and NMR signal, cm 3;VH1 is a water volume filled in the sample tube, cm 3;SH1 is an NMR signal of water corresponding to the liquid filling amount, and the unit is dimensionless.
2) Step 2 of the preparation stage: for the F probe, measuring the volume V F1 of the fluorine-added liquid FC-40 in the nuclear magnetic resonance signal linear region range of the sample tube by a weighing method, and measuring the NMR signal S F1 of the F element at the moment, thereby obtaining the scale coefficient of the volume of the fluorine-added liquid FC-40 and the nuclear magnetic resonance signal: k F= VF1/ SF1, wherein K F is the scale factor of the volume of the fluorinated liquid FC-40 and the nuclear magnetic resonance signal, the unit cm 3;VF1 is the volume of the fluorinated liquid FC-40 in the sample tube, the unit cm 3;SF1 is the NMR signal of the fluorinated liquid FC-40 when the liquid adding amount corresponds, and the unit is dimensionless.
3) Step 3 of the preparation stage: aiming at the F probe, continuously adding the fluorinated liquid FC-40 into the sample tube until the nuclear magnetic resonance signal quantity is not increased any more, obtaining the maximum nuclear magnetic resonance signal quantity S Fmax when the sample tube is only added with the fluorinated liquid FC-40, and making a liquid adding liquid level line mark of the maximum value of the F signal.
4) Test of sample to be tested step 1: cleaning a sample to be tested by wet filter paper, filling the sample into a sample tube (the filling height of the sample is lower than the upper limit of a nuclear magnetic resonance signal linear region), and then adding a fluorinated liquid FC-40 into the sample tube, wherein the filling height of the fluorinated liquid is higher than a filling liquid level line of the maximum value of an F signal; after the liquid adding is finished, a sealing cover is screwed on the sample tube, a centrifuge is put in, the sample is centrifuged at proper rotation speed and time, and residual fluid on the surface of the sample to be detected is stripped from the surface by virtue of centrifugal force by utilizing the physical characteristics of the fluoridized liquid FC-40 with density (1.85 g/cm 3) > water (1 g/cm 3), so that the influence of a water film on the surface of the sample to be detected on pore volume measurement is reduced; after centrifugation is completed, the sample tube to be measured is filled into a nuclear magnetic resonance instrument, and a nuclear magnetic resonance signal S H2 is measured by using an H probe to obtain the pore volume of the sample to be measured: Wherein V por is the pore volume of the sample to be measured, cm 3;SH2 is the NMR signal of the sample to be measured in the H probe, and the unit is dimensionless; k H is the water volume and the scale factor of the NMR signal, unit cm 3.
5) Step 2, testing a sample to be tested: the sample after the step 1 is finished is not processed, the sample is placed into an F probe of an NMR measuring instrument, the NMR signal S F2.SF2<SFmax of the F element is measured, the signal difference of the sample skeleton and the pore volume which do not contribute to the NMR signal of the F element is obtained, and therefore the apparent volume (namely the total volume) of the sample to be measured can be calculated: wherein V T is the total volume of the sample to be measured, cm 3;SFmax is the maximum F signal quantity of the sample tube when only the fluoride solution FC-40 is added, and the unit is dimensionless; s F2 is the NMR signal quantity of F element after loading the sample to be tested and adding the fluoride solution FC-40, and the unit is dimensionless.
The pore volume and the total volume of the sample to be measured are obtained through 2 steps of measurement (a H, F element probe is used in sequence), and the porosity of the sample to be measured is as follows:
。
Compared with the NMR-H probe rock chip porosity measurement method, the NMR-H, F probe rock chip porosity measurement method has the advantage that errors caused by incomplete removal of surface fluid by a wiping method of a sample to be measured are solved through fluid density difference. The characteristic that the NMR probe has the maximum signal quantity is skillfully utilized, and the concave liquid level error existing in the fixed liquid adding quantity is solved. But the introduction of the F probe also results in more complex NMR equipment and the increased centrifugation step of the sample tube also reduces the efficiency of the test. Whether the centrifugal force is proper or not can influence the measurement result, and too large centrifugal force can cause the pore fluid of the sample to be measured to be thrown out, so that the pore volume measurement value is smaller; if the centrifugal force is too small, the effect of stripping the fluid on the surface of the sample to be tested can not be achieved; the viscosity difference of the residual drilling mud slurry on the surface of the sample to be tested makes the centrifugal operation effect more difficult to guarantee.
In conclusion, the nuclear magnetic resonance-density balance method has low speed measurement, complex operation and no acceptance in industry, and is not suitable for granular rock debris samples. The NMR-H probe rock debris porosity measurement method and the NMR-H, F probe rock debris porosity measurement method developed in recent years have a great breakthrough, but have a plurality of defects.
Therefore, it is desirable to provide a new testing method and apparatus for irregularly shaped cores to solve the above-mentioned problems.
Disclosure of Invention
The present invention aims to solve at least one of the technical problems existing in the prior art. Therefore, the invention provides the method and the device for testing the porosity of the irregular-shaped core, which can realize the on-site rapid and high-precision testing of the porosity of the irregular-shaped core such as the sidewall coring core and the drilling cuttings by using the drilling fluid, and are simple and easy to operate.
In a first aspect, the present application provides a method for testing porosity of an irregularly shaped core, the method comprising:
placing a volume scale sample into a sample tube and not exceeding a first mark line of the sample tube, testing to obtain a nuclear magnetic resonance signal S H1 of the volume scale sample, and calculating to obtain a scale coefficient K H,KH=VH/SH1,VH of the volume scale sample as the volume of hydrogen-containing liquid of the volume scale sample, wherein a region between the first mark line of the sample tube and the bottom of the sample tube corresponds to a nuclear magnetic resonance signal linear region;
Taking out the volume scale standard sample, adding the hydrogen-containing liquid into the sample tube until the liquid adding height is between a second mark line and a third mark line of the sample tube, and testing to obtain a nuclear magnetic resonance signal S Hmax of the hydrogen-containing liquid, wherein the region between the first mark line and the second mark line corresponds to a nuclear magnetic resonance signal nonlinear region, and the region between the second mark line and the third mark line corresponds to a highest nuclear magnetic resonance signal region;
Pretreating a sample to be detected, placing the pretreated sample to be detected into a sample tube and not exceeding a first marking line of the sample tube, testing to obtain a nuclear magnetic resonance signal S H2 of the sample to be detected, and calculating to obtain the pore volume V por,Vpor=KH×SH2 of the sample to be detected;
Adding the hydrogen-containing liquid into the sample tube in which the sample to be detected is placed until the liquid adding height is between the second mark line and the third mark line of the sample tube, testing to obtain nuclear magnetic resonance signals S H3 of the sample to be detected and the hydrogen-containing liquid, and calculating to obtain skeleton volume V G,VG=KH×(SHmax-SH3 of the sample to be detected;
Calculating to obtain the porosity of the sample to be measured ，
。
Further, the method for acquiring the second mark line includes:
And taking out the volume scale standard sample, continuously adding the hydrogen-containing liquid into the sample tube until the nuclear magnetic resonance signal of the hydrogen-containing liquid is maximum, wherein the liquid level surface corresponding to the maximum nuclear magnetic resonance signal of the hydrogen-containing liquid is the second mark line.
Further, the preprocessing of the sample to be detected includes: and removing the fluid on the surface of the sample to be detected.
Preferably, the preprocessing the sample to be tested includes: and wiping the fluid on the surface of the sample to be tested by using wet filter paper.
Further, a CPMG sequence is employed to acquire the nuclear magnetic resonance signal.
Further, the hydrogen-containing liquid is a copper sulfate solution with the mass concentration of 1000-1500 ppm.
Further, the adding the hydrogen-containing liquid into the sample tube in which the sample to be measured is placed until the liquid adding height is between the second mark line and the third mark line of the sample tube includes:
And eliminating bubbles adsorbed on the surface of the sample to be detected.
Preferably, the adding the hydrogen-containing liquid into the sample tube in which the sample to be measured is placed until the liquid adding height is between the second mark line and the third mark line of the sample tube includes:
and (3) holding the sample tube to lightly throw in one direction, so that the sample to be tested slightly vibrates at the bottom of the sample tube, and eliminating bubbles adsorbed on the surface of the sample to be tested.
In a second aspect, the present application also provides an apparatus for the porosity testing method of the irregularly shaped core, where the apparatus includes: the device comprises a magnet unit, a radio frequency unit, a spectrometer unit, a calculation unit and a sample tube;
The magnet unit comprises a magnet which is used for providing a magnetic field for the volume scale standard sample, the hydrogen-containing liquid and the sample to be tested, and the magnetic field strength of the magnet is 0.1-0.2T;
The radio frequency unit is used for detecting nuclear magnetic resonance signals of the volume calibration standard sample, the hydrogen-containing liquid and the sample to be detected, the radio frequency unit comprises a radio frequency coil, the radio frequency coil is an H radio frequency coil with low filling sensitivity, the radio frequency coil is provided with a nuclear magnetic resonance signal linear region, a nuclear magnetic resonance signal nonlinear region and a highest nuclear magnetic resonance signal region, when the liquid level surface of the hydrogen-containing liquid is in the nuclear magnetic resonance signal linear region, the nuclear magnetic resonance signals of the hydrogen-containing liquid are in direct proportion to the volume of the hydrogen-containing liquid, when the liquid level surface of the hydrogen-containing liquid is in the nuclear magnetic resonance signal nonlinear region, the nuclear magnetic resonance signals of the hydrogen-containing liquid and the volume of the hydrogen-containing liquid are in a nonlinear monotonically increasing rule, when the liquid level surface of the hydrogen-containing liquid is in the highest nuclear magnetic resonance signal region, the nuclear magnetic resonance signals of the hydrogen-containing liquid reach the maximum value, and the nuclear magnetic resonance signal deviation of the hydrogen-containing liquid in the highest nuclear magnetic resonance signal region is less than or equal to +/-1%;
The spectrometer unit is used for controlling the radio frequency unit to collect nuclear magnetic resonance signals of the volume scale standard sample, the hydrogen-containing liquid and the sample to be detected;
the computing unit is used for computing the porosity of the sample to be tested;
The sample tube is used for placing the volume scale standard sample, the hydrogen-containing liquid and the sample to be measured in the radio frequency coil, a first mark line, a second mark line and a third mark line are arranged on the surface of the sample tube, the region between the first mark line and the bottom of the sample tube corresponds to the nuclear magnetic resonance signal linear region, the region between the first mark line and the second mark line corresponds to the nuclear magnetic resonance signal nonlinear region, and the region between the second mark line and the third mark line corresponds to the highest nuclear magnetic resonance signal region.
Further, the inductance range of the radio frequency coil is as follows。
Further, the sample tube comprises a main body and a sealing cover, wherein the main body is of a cylinder structure with one end being open, the main body and the sealing cover form an accommodating space, the accommodating space is used for accommodating a volume scale standard sample, hydrogen-containing liquid and a sample to be tested, an internal thread is arranged at an opening of the main body, the sealing cover is provided with an external thread matched with the internal thread for use, and the sealing cover can move along a preset direction through the internal thread to seal the main body.
Further, knurling is arranged on the surface of the sealing cover, and one end, far away from the opening, of the main body is arc-shaped.
The above-described one or more embodiments of the present invention have at least one or more of the following advantages:
The application provides a porosity testing method and device for an irregularly-shaped rock core, which are characterized in that firstly, the pore volume of a sample to be tested is obtained through testing, then hydrogen-containing liquid is added into a sample tube filled with the sample to be tested to a highest nuclear magnetic resonance signal area, nuclear magnetic resonance signals of the sample to be tested and the hydrogen-containing liquid are obtained through testing, the skeleton volume of the sample to be tested is obtained through calculation by utilizing a scale curve, and finally, the porosity of the sample to be tested is obtained through using the pore volume and the skeleton volume. According to the method provided by the application, when the skeleton volume of the sample to be tested is tested, the sample is not required to be transferred, so that the test efficiency is improved, and the problem of large test error of the skeleton volume caused by the fact that the sample is blocked or particles fall in the transfer process is avoided. In addition, the application adopts the nuclear magnetic resonance method to test the skeleton volume of the sample to be tested, and can improve the testing accuracy of the skeleton volume of the small-particle rock debris sample, thereby improving the testing accuracy of the porosity of the small-particle rock debris sample.
Further, the radio frequency coil provided by the application is an H radio frequency coil with low filling sensitivity, and the H radio frequency coil is provided with a nuclear magnetic resonance signal linear region, a nuclear magnetic resonance signal nonlinear region and a highest nuclear magnetic resonance signal region, when the liquid level surface of the hydrogen-containing liquid is in the nuclear magnetic resonance signal linear region, the nuclear magnetic resonance signal of the hydrogen-containing liquid is in direct proportion to the volume of the hydrogen-containing liquid, when the liquid level surface of the hydrogen-containing liquid is in the nuclear magnetic resonance signal nonlinear region, the nuclear magnetic resonance signal of the hydrogen-containing liquid and the volume of the hydrogen-containing liquid are in a nonlinear monotonically increasing rule, when the liquid level surface of the hydrogen-containing liquid is in the highest nuclear magnetic resonance signal region, the nuclear magnetic resonance signal of the hydrogen-containing liquid reaches the maximum value, and the nuclear magnetic resonance signal deviation of the hydrogen-containing liquid in the highest nuclear magnetic resonance signal region is less than or equal to +/-1%. Because the H radio frequency coil has the characteristics, the hydrogen-containing liquid is only required to be added to the highest nuclear magnetic resonance signal zone when the skeleton volume of the sample to be tested is tested, so that the constraint that the skeleton volume of the sample to be tested, which is tested by adding the hydrogen-containing liquid, must be added to a fixed liquid level line is avoided. Therefore, the method and the device provided by the application can improve the porosity test precision and reduce the operation difficulty. In addition, the porosity of the sample to be tested can be accurately and rapidly tested by using the H radio frequency coil, so that the price of a nuclear magnetic resonance instrument is reduced, and the popularization of the testing method and the device provided by the application is facilitated.
Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
Drawings
The present disclosure will become more readily understood with reference to the accompanying drawings. As will be readily appreciated by those skilled in the art: the drawings are for illustrative purposes only and are not intended to limit the scope of the present invention. Moreover, like numerals in the figures are used to designate like parts, wherein:
FIG. 1 is a flow chart of a method for testing the porosity of an irregularly shaped core provided by the present application;
FIG. 2 is a schematic illustration of a method for testing the porosity of irregularly shaped cores provided by the present application;
FIG. 3 is a frame diagram of an apparatus for the porosity testing method for irregularly shaped cores provided by the present application;
FIG. 4 is a schematic diagram of the relationship between the volume of hydrogen-containing liquid added to a sample tube of the porosity testing device for irregular-shaped cores and nuclear magnetic resonance signals;
FIG. 5 is a schematic representation of the relationship between the volume of hydrogen-containing liquid added to a sample tube of a prior art porosity testing device and nuclear magnetic resonance signals;
Fig. 6 is a physical view of a sample tube provided by the present application.
Detailed Description
Some embodiments of the invention are described below with reference to the accompanying drawings. It should be understood by those skilled in the art that these examples are merely for explaining the technical principles of the present invention and are not intended to limit the scope of the present invention.
As shown in the background art, when the porosity of the irregularly-shaped rock core such as the sidewall coring rock core and the drilling rock scraps is tested by adopting a drying method, the defects of poor testing accuracy, low testing efficiency, environmental pollution caused by drying hydrocarbon components in a sample, harm to the body of a tester and the like exist; although the nuclear magnetic resonance-density balance method solves the problems of hydrocarbon drying pollution and the like, the nuclear magnetic resonance-density balance method also has the problems of complex operation, poor testing accuracy, low testing efficiency and the like; by adopting an NMR-H probe rock debris porosity measurement method, although a sample is not required to be transferred in the middle test process, the measurement accuracy of the skeleton volume is limited due to human error of the concave liquid level when a sample tube is added with liquid; although the NMR-H, F probe rock debris porosity measurement method can solve the concave liquid level error existing in the fixed liquid filling amount, the introduction of the F probe also causes the nuclear magnetic resonance equipment to be more expensive and complicated.
In this regard, the application creatively provides a porosity testing method and device for an irregularly-shaped core, and the sample is not required to be transferred when the skeleton volume of the sample to be tested is tested, so that the testing efficiency is improved, and the problem that the large testing error exists in the skeleton volume due to the fact that the sample is blocked or particles fall in the transferring process is avoided. In addition, the application adopts the nuclear magnetic resonance method to test the skeleton volume of the sample to be tested, and can improve the testing accuracy of the skeleton volume of the small-particle rock debris sample, thereby improving the testing accuracy of the porosity of the small-particle rock debris sample. The H radio frequency coil provided by the application is low-filling-sensitivity, and only the hydrogen-containing liquid is required to be added to the highest nuclear magnetic resonance signal zone when the skeleton volume of the sample to be tested is tested, so that the constraint that the skeleton volume of the sample to be tested is required to be added to a fixed liquid level line when the hydrogen-containing liquid is added is avoided. In addition, the porosity of the sample to be tested can be obtained by testing only using the H radio frequency coil, so that the price of a nuclear magnetic resonance instrument is reduced, and the popularization of the testing method and the device provided by the application is facilitated.
The following is an optional technical scheme of the present application, but not limiting the technical scheme provided by the present application, and the technical purpose and beneficial effects of the present application can be better achieved and achieved through the following optional technical scheme.
In a first aspect, the present application provides a method for testing the porosity of an irregularly shaped core, as shown in fig. 1, where the method includes:
S1: and placing a volume calibration standard sample into a sample tube and not exceeding a first mark line of the sample tube, testing to obtain a nuclear magnetic resonance signal S H1 of the volume calibration standard sample, and calculating to obtain a calibration coefficient K H,KH=VH/SH1,VH of the volume calibration standard sample as the volume of the hydrogen-containing liquid of the volume calibration standard sample, wherein a region between the first mark line of the sample tube and the bottom of the sample tube corresponds to a nuclear magnetic resonance signal linear region.
It should be noted here that at least 3-4 hours in advance of the drilling fluid field test are needed to prepare the drilling fluid in the field. Firstly, a nuclear magnetic resonance instrument is unfolded, a power supply is turned on, the magnet is turned on for temperature control, and the magnet temperature is kept stable until reaching a set value. And then, after the temperature of the magnet is stable, starting the power supply of the instrument electronic cabinet and the data acquisition computer, and starting the data acquisition software to preheat the whole system by using the fid sequence for half an hour. And finally, after the whole machine of the instrument is preheated, calibrating the instrument, searching the center frequency of the magnet, the radio frequency excitation parameters and the like, and acquiring nuclear magnetic resonance signals by adopting a CPMG sequence after the instrument is determined to reach a stable state. Specifically, the gain parameters of the instrument are fixed, the waiting time TW, the echo interval TE, the echo number NECH and the accumulation times NS of the acquisition parameters of the CPMG sequence are set, the nuclear magnetic resonance signals are tested by using volume calibration standards configured along with the instrument, and the calibration coefficient K H of the hydrogen-containing liquid volume and the nuclear magnetic resonance signals is obtained.
Specifically, as shown in fig. 2 (a), the volume calibration standard sample 200 is first placed in the sample tube and does not exceed the first mark line 110 of the sample tube, then the sample tube is placed in the radio frequency coil detection area, the nuclear magnetic resonance signal S H1 of the volume calibration standard sample 200 is obtained by testing, and the calibration coefficient K H,KH=VH/SH1,VH of the volume calibration standard sample 200 is calculated to be the volume of the hydrogen-containing liquid of the volume calibration standard sample 200. The region between the first mark line 110 of the sample tube and the bottom of the sample tube corresponds to the nmr signal linear region 10, where the nmr signal linear region 10 refers to that when the level surface of the hydrogen-containing liquid is in the region, the nmr signal of the hydrogen-containing liquid is proportional to the volume of the hydrogen-containing liquid, i.e., as the volume of the hydrogen-containing liquid increases, the nmr signal thereof is in a linear monotonic increasing rule.
In the present application, the volume calibration standard 200 is a sample of known volume of hydrogen-containing liquid. As a preferred embodiment, a known volume of hydrogen-containing liquid is sealed in a container to form the volume calibration standard 200, so that the deviation of the calibration coefficient K H caused by volatilization of the hydrogen-containing liquid in the volume calibration standard 200 during use is avoided.
In a specific embodiment, the hydrogen-containing liquid in the volume calibration standard 200 is a copper sulfate solution with a mass concentration of 1000-1500ppm, preferably, the hydrogen-containing liquid in the volume calibration standard 200 is a copper sulfate solution with a mass concentration of 1000ppm, and the relaxation time of T 2 of the hydrogen-containing liquid in a nuclear magnetic resonance apparatus under the corresponding magnetic field strength is about 100 ms. The reason for using the copper sulfate solution is that the relaxation time of the pure water is about 2-3 seconds, and the required nuclear magnetic resonance acquisition time is too long, which affects the test efficiency, so that the relaxation time of the copper sulfate solution can be shortened, and the sampling time can be shortened.
S2: and taking out the volume scale standard sample, adding the hydrogen-containing liquid into the sample tube until the liquid adding height is between a second mark line and a third mark line of the sample tube, and testing to obtain a nuclear magnetic resonance signal S Hmax of the hydrogen-containing liquid, wherein the region between the first mark line and the second mark line corresponds to a nuclear magnetic resonance signal nonlinear region, and the region between the second mark line and the third mark line corresponds to a highest nuclear magnetic resonance signal region.
The non-linear region of the nmr signal refers to that when the hydrogen-containing liquid 300 is added in the sample tube until the liquid level surface thereof is in the non-linear region of the nmr signal, the nmr signal of the hydrogen-containing liquid 300 and the volume of the hydrogen-containing liquid 300 are in a non-linear monotonically increasing rule. The highest nuclear magnetic resonance signal zone means that when the hydrogen-containing liquid 300 is added in the sample tube until the liquid level surface is in the highest nuclear magnetic resonance signal zone, the nuclear magnetic resonance signal of the hydrogen-containing liquid 300 reaches the maximum value, and the nuclear magnetic resonance signal deviation of the hydrogen-containing liquid 300 in the highest nuclear magnetic resonance signal zone is less than or equal to +/-1%. In the present application, the region between the first marker line 110 and the second marker line 120 corresponds to the nuclear magnetic resonance signal nonlinear region 20, and the region between the second marker line 120 and the third marker line 130 corresponds to the highest nuclear magnetic resonance signal region 30.
Further, the method for acquiring the second mark line includes: as shown in fig. 2 (b), the volume calibration standard 200 is taken out, and the hydrogen-containing liquid 300 is continuously added into the sample tube until the nuclear magnetic resonance signal of the hydrogen-containing liquid 300 is maximum, and the liquid level surface corresponding to the maximum nuclear magnetic resonance signal of the hydrogen-containing liquid 300 is the second mark line 120.
It should be noted that, step S1 and step S2 are only required to be performed once before a batch of samples to be tested are tested, and step S1 and step S2 are volume scales of nuclear magnetic resonance signals and detection of maximum signal quantity.
S3: pretreating a sample to be detected, placing the pretreated sample to be detected into the sample tube and not exceeding a first marking line of the sample tube, testing to obtain a nuclear magnetic resonance signal S H2 of the sample to be detected, and calculating to obtain the pore volume V por,Vpor=KH×SH2 of the sample to be detected.
In order to ensure the accuracy of the test, the working state of the nuclear magnetic resonance instrument needs to be detected before the sample to be tested is tested, so as to ensure that the nuclear magnetic resonance instrument works normally. Using polytetrafluoroethylene block with known volume (regular cylinder, measuring volume V PTFE1) configured with instrument, placing into dried sample tube, then adding hydrogen-containing liquid (liquid level surface of hydrogen-containing liquid exceeds nuclear magnetic resonance signal nonlinear region) configured in step S2, placing the filled sample tube into radio frequency coil detection region, adopting nuclear magnetic resonance acquisition parameter identical to that in step S2, measuring nuclear magnetic resonance signal S PTFE, using the invented method to calculate its volumeIf the relative error between V PTFE2 and V PTFE1 is less than or equal to 3%, the instrument is normal in function, and the on-site sample to be tested can be tested.
Further, the pretreatment of the sample to be tested comprises: and removing the fluid on the surface of the sample to be detected. As a preferred embodiment, the fluid on the surface of the sample to be tested is wiped with wet filter paper to avoid the influence of the fluid on the surface of the sample to be tested on the test result. In addition, for the sidewall coring core and cuttings samples, because the surface generally has drilling mud residues, the surface needs to be washed with clean water before measurement so as to avoid influencing the test result with mud testing.
Further, as shown in fig. 2 (c), the pretreated sample 400 to be measured is placed in the sample tube and does not exceed the first marking line 110 of the sample tube, the nuclear magnetic resonance signal S H2 of the sample to be measured is obtained by testing, and the pore volume V por,Vpor=KH×SH2 of the sample to be measured is calculated.
S4: and adding the hydrogen-containing liquid into the sample tube in which the sample to be detected is placed until the liquid adding height is between the second mark line and the third mark line of the sample tube, testing to obtain nuclear magnetic resonance signals S H3 of the sample to be detected and the hydrogen-containing liquid, and calculating to obtain the skeleton volume V G,VG=KH×(SHmax-SH3 of the sample to be detected.
Specifically, as shown in fig. 2 (d), the hydrogen-containing liquid 300 configured in step S2 is added into the sample tube in which the sample 400 is placed until the liquid filling height is between the second marker line 120 and the third marker line 130 of the sample tube, then the sample tube in which the sample 400 is placed into the radio frequency coil detection area, the nuclear magnetic resonance signals S H3 of the sample 400 and the hydrogen-containing liquid 300 are obtained through testing, and the skeleton volume V G,VG=KH×(SHmax-SH3 of the sample is calculated.
In the process of adding hydrogen-containing liquid into a sample tube, bubbles usually adhere to the surface of the sample due to the action of surface tension, and if bubbles adsorbed on the surface of the sample are not removed, the volume occupied by the bubbles can cause the framework to be larger, so that the porosity measurement value is lower. To solve this problem, adding the hydrogen-containing liquid 300 to the sample tube in which the sample 400 to be measured is placed until the filling height is between the second marker line 120 and the third marker line 130 of the sample tube includes: removing the fluid on the surface of the sample 400 to be measured. Specifically, the sample tube is gripped and thrown in one direction, so that the sample 400 to be measured slightly vibrates at the bottom of the sample tube, and bubbles adsorbed on the surface of the sample 400 to be measured are removed. Through the operation, the bubbles adsorbed on the surface of the sample can be removed in time, so that the skeleton volume test of the sample is more accurate, and the test precision of the porosity can be improved.
It should be noted that the sampling parameters of the nmr signal are kept as consistent as possible throughout the test, and in particular, the cumulative Number (NS) and the echo Time (TE) should be kept consistent. If a sample with longer T 2 relaxation time is encountered, only the waiting Time (TW) and the Number of Echoes (NECH) are required to be adjusted, so that the fluid signal in the sample is fully relaxed. Since the sample 400 to be measured generally has micro-nano pores, the minimum value of the nmr is required for the echo interval TE to ensure the measurement accuracy.
In addition, in step S2, because the radio frequency coil is required to be used in the test to detect the state that the area is filled with the hydrogen-containing liquid, the nuclear magnetic resonance signal is the largest at this time, in order to avoid saturation of the instrument signal, the gain parameter of the instrument is required to be reasonably set, and a larger gain parameter is adopted as much as possible on the premise of ensuring that the nuclear magnetic resonance signal is unsaturated, so as to ensure the data signal to noise ratio when the nuclear magnetic resonance signal is acquired by the sample with the lower signal quantity. It is recommended to fix the instrument gain parameters during the test, if the gain parameters are not fixed (for example, small gain is used to avoid signal saturation during the test of hydrogen-containing liquid, large gain is used to ensure high signal to noise ratio during the test of the sample to be tested), and gain correction is performed on the nuclear magnetic resonance signal during the calculation of the porosity.
S5: calculating to obtain the porosity of the sample to be measured，
。
After all samples 400 to be tested are tested, the hydrogen-containing liquid 300 is sent to a chemical waste recovery tank or a recovery pool on a drilling site, and the samples cannot be poured at will; and processing data, sorting test reports, closing a nuclear magnetic resonance instrument power supply, and accommodating a sample tube, a power line, a notebook computer and the like.
In a second aspect, the present application further provides an apparatus for the method for testing the porosity of the irregularly shaped core, as shown in fig. 3, where the apparatus includes: a magnet unit, a radio frequency unit, a spectrometer unit 3000, a calculation unit 4000 and a sample tube 5000.
The radio frequency unit is used for detecting nuclear magnetic resonance signals of the volume scale standard sample, the hydrogen-containing liquid and the sample to be detected. Specifically, the rf unit includes an rf coil 2100, an rf power amplifier 2200, an energy release module 2300, a TR switch 2400, a coupler 2500, a preamplifier 2600, and a dual-channel rf switch 2700. The rf coil 2100 is used to emit rf pulses to excite H nuclei in the sample to generate nmr signals, and to receive nmr signals from H nuclei in the sample, and thus is also the location to load the sample tube 5000; the rf power amplifier 2200 amplifies the rf excitation signal power of the spectrometer unit 3000 to generate an rf excitation pulse with sufficient power; the energy discharging module 2300 is used for rapidly discharging the radio frequency energy after the excitation is finished, reducing the acquisition preparation time of a radio frequency unit and further realizing a short echo interval sampling function; the TR switch 2400 functions as a key device for rapidly switching the excitation and reception modes of the radio frequency coil 2100; the coupler 2500 and the dual-channel radio frequency switch 2700 are used for receiving and transmitting nuclear magnetic signals, and the resonance characteristics of the radio frequency coil 2100 are checked; the pre-amplifier 2600 functions as an analog signal amplifier that amplifies the weak nuclear magnetic signal of the sample to improve the key device of the signal-to-noise ratio of the sampled data.
Unlike prior art nmr instruments, the rf coil 2100 of the present application has low sensitivity characteristics to reduce the amount of change in resonant frequency of the rf coil 2100 when a hydrogen-containing liquid is continuously added during the testing of the volume of the bobbin. Specifically, the rf coil 2100 has a linear region of nuclear magnetic resonance signal, a nonlinear region of nuclear magnetic resonance signal, and a highest nuclear magnetic resonance signal region, when the level surface of the hydrogen-containing liquid is in the linear region of nuclear magnetic resonance signal, the nuclear magnetic resonance signal of the hydrogen-containing liquid is proportional to the volume of the hydrogen-containing liquid, when the level surface of the hydrogen-containing liquid is in the nonlinear region of nuclear magnetic resonance signal, the nuclear magnetic resonance signal of the hydrogen-containing liquid and the volume of the hydrogen-containing liquid are in a nonlinear monotonically increasing rule, when the level surface of the hydrogen-containing liquid is in the highest nuclear magnetic resonance signal region, the nuclear magnetic resonance signal of the hydrogen-containing liquid reaches a maximum value, and the nuclear magnetic resonance signal deviation of the hydrogen-containing liquid in the highest nuclear magnetic resonance signal region is less than or equal to ±1%.
In the present application, a sample tube 5000 to which a hydrogen-containing liquid is added is placed in a radio frequency coil 2100, and the relationship between the nuclear magnetic resonance signal and the volume of the hydrogen-containing liquid is shown in fig. 4. When the liquid level surface of the hydrogen-containing liquid is in the nuclear magnetic resonance signal linear region 10, the nuclear magnetic resonance signal of the hydrogen-containing liquid is proportional to the volume of the hydrogen-containing liquid; when the liquid level surface of the hydrogen-containing liquid is in the nuclear magnetic resonance signal nonlinear region 20, the nuclear magnetic resonance signal of the hydrogen-containing liquid and the volume of the hydrogen-containing liquid are in a nonlinear monotonic increasing rule, when the liquid level surface of the hydrogen-containing liquid is in the highest nuclear magnetic resonance signal region 30, the nuclear magnetic resonance signal of the hydrogen-containing liquid reaches the maximum value, and the nuclear magnetic resonance signal deviation of the hydrogen-containing liquid in the highest nuclear magnetic resonance signal region is less than or equal to +/-1%. When only the nuclear magnetic resonance signal quantity and the volume of the hydrogen-containing liquid are shown as the characteristics shown in figure 4, the specific liquid level surface is not required to be aligned when the hydrogen-containing liquid is added to test the skeleton volume of the sample to be tested, and only the liquid level surface of the hydrogen-containing liquid is required to be in the highest nuclear magnetic resonance signal area, so that the design targets of convenient operation, small human error and the like are achieved. Therefore, the method and the device provided by the application can improve the porosity test precision and reduce the operation difficulty.
The rf coil design objective of the nmr apparatus in the prior art only needs to use the first region 40 (the first region 40 corresponds to the linear region of the nmr signal, in which the nmr signal is proportional to the volume of the hydrogen-containing liquid) in fig. 5, so as to achieve the purpose of quantitative calculation, so that the loading height of the nmr apparatus in the prior art during testing does not exceed the first region 40. When the rf coil of such nmr apparatus is directly used in the measurement of the present invention without the improvement of design, the phenomenon shown in fig. 5 is generally encountered, and as known from the working principle of the present invention, the response characteristics of the nmr signal and the liquid adding amount in fig. 5 cannot be used in the method of the present invention. The fundamental reason for the phenomenon shown in fig. 5 is that the resonance characteristic of the rf coil changes after the filling amount exceeds a certain range due to the high filling sensitivity of the rf coil, and the rf coil is in a polarized state, so that the nmr signal amount is smaller than a normal value.
To achieve the rf coil response characteristics shown in fig. 4, targeted modifications to the rf coil are required, such as: the distributed capacitance is increased when the radio frequency coil is wound, the Q value is properly reduced, and the filling sensitivity of the radio frequency coil is reduced. In the application, the radio frequency coil is an H radio frequency coil with low filling sensitivity, and the inductance range of the radio frequency coil is preferably. The porosity of the sample to be tested can be accurately and rapidly tested by using the H radio frequency coil, so that the price of a nuclear magnetic resonance instrument is reduced, and the popularization of the testing method and the device provided by the application is facilitated.
The magnet unit includes a magnet 1100 and a temperature controller 1200, and the temperature controller 1200 is used to control the temperature of the magnet 1100 to be stabilized within a certain range. The magnet 1100 is used for providing a magnetic field for a volume calibration standard sample, a hydrogen-containing liquid and a sample to be tested, the magnetic field strength of the magnet 1100 also has an effect on the filling sensitivity of the radio frequency coil 2100, the lower the magnetic field strength of the magnet 1100 is, the smaller the filling sensitivity of the radio frequency coil 2100 is, but the lower the magnetic field strength of the magnet 1100 is, the signal-to-noise ratio of nuclear magnetic data is also reduced. In order to improve the signal-to-noise ratio of the nuclear magnetic data while taking account of the low sensitivity characteristic of the rf coil 2100, it is verified that the magnetic field strength of the magnet 1100 is 0.1-0.2T in the present invention, and preferably the magnetic field strength of the magnet 1100 is 0.14T (the corresponding H nuclear resonance frequency is 6 MHz) in the present invention.
Further, the spectrometer unit 3000 is used for controlling the radio frequency unit to collect nuclear magnetic resonance signals of the volume calibration standard sample, the hydrogen-containing liquid and the sample to be measured. The computing unit 4000 is used for computing the porosity of the sample to be tested, and specifically, the computing unit 4000 consists of a collecting computer and corresponding software.
Sample tube 5000 is used to place volume calibration standards, hydrogen-containing fluids, and samples to be tested in radio frequency coil 2100. In order to improve the test efficiency, as shown in fig. 6, the surface of the sample tube is notched with the first marker line 110, the second marker line 120 and the third marker line 130 according to the test result of the radio frequency coil, the region between the first marker line 110 and the bottom of the sample tube corresponds to the linear region of the nuclear magnetic resonance signal, the region between the first marker line 110 and the second marker line 120 corresponds to the nonlinear region of the nuclear magnetic resonance signal, and the region between the second marker line 120 and the third marker line 130 corresponds to the region of the highest nuclear magnetic resonance signal. The position of the liquid level surface when the hydrogen-containing liquid is added is conveniently observed and controlled through grooving. The first mark line 110 is the upper limit of the loading height of the sample to be tested, the second mark line 120 is the lowest level surface when the hydrogen-containing liquid is added, the third mark line 130 is the highest level surface when the hydrogen-containing liquid is added, and the third mark line 130 is designed to avoid too much hydrogen-containing liquid being added, exposing the rf coil waveguide and introducing external electromagnetic interference.
Further, the sample tube comprises a main body 100 and a sealing cover 200, wherein the main body 100 is of a cylinder structure with one end open, the main body 100 and the sealing cover 200 form an accommodating space, and the accommodating space is used for accommodating a volume scale sample, a hydrogen-containing liquid and a sample to be measured. The opening part of main part is provided with the internal screw thread, and sealed lid is provided with the external screw thread that uses with the internal screw thread cooperation, and sealed lid 200 can follow the direction of predetermineeing through the internal screw thread and remove in order to seal main part 100, and this sealed lid 200 can delay the volatile effect that awaits measuring sample contact air, can avoid the hydrogen-containing liquid spill pollution radio frequency coil when the test again after the sample cell adds the hydrogen-containing liquid. In addition, the surface of the sealing cover 200 is provided with knurling, so that the sampling tube can be conveniently taken out of the radio frequency coil. In order to improve the testing efficiency, the end of the main body 100 away from the opening is in a circular arc shape, that is, the bottom of the sample tube is in a circular arc shape similar to the bottom of a thermos bottle, so that the sample tube and the residual hydrogen-containing liquid at the bottom can be quickly wiped after the tested sample is poured out, and the next sample to be tested can be tested. In order to avoid the introduction of nuclear magnetic resonance signals, the sample tube is made of polytetrafluoroethylene which is not fragile and easy to deform and has no nuclear magnetic resonance signals.
In order to further improve the testing efficiency, the sample tubes are manufactured by adopting precise machining, the internal dimensional accuracy is controlled, 3-5 sample tubes with the relative value of K H、SHmax value difference less than or equal to 1% are screened out as 1 group by utilizing the measuring preparation process in the invention after molding, and the sample tubes are matched with 1 nuclear magnetic resonance instrument for use, so that the subsequent samples to be tested can be loaded in advance by utilizing the measuring waiting time during on-site operation.
In addition, in order to facilitate the reciprocating transportation of the drilling site, the device provided by the application adopts a portable structural design.
Embodiments of the present invention will be described more specifically below by way of examples. However, embodiments of the present invention are not limited to these examples only.
The following examples are illustrative only and are not to be construed as limiting the application. The examples are not to be construed as limiting the specific techniques or conditions described in the literature in this field or as per the specifications of the product. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
Example 1
In order to verify the accuracy of the method provided by the invention, a verification test is designed: the polytetrafluoroethylene cylindrical thin sheets with consistent sizes are processed, the measurement volume of each sheet is 4.13cm 3, and different numbers of polytetrafluoroethylene cylindrical thin sheets are added into a sample tube. Because the polytetrafluoroethylene does not contain nuclear magnetic resonance signals, the method provided by the invention is used for measuring the volume of the polytetrafluoroethylene cylindrical sheet added into the sample tube, the test result is compared with a ruler method, the test result is shown in the table 1, and the relative error of the polytetrafluoroethylene cylindrical sheet tested by the method and the polytetrafluoroethylene cylindrical sheet measured by the ruler method is less than or equal to 2%, so that the feasibility of the method provided by the invention is verified.
TABLE 1 results of volume testing of cylindrical polytetrafluoroethylene sheets
Example 2
The porosity of the block-shaped sidewall coring core sample is tested by using the method provided by the invention in the X well of the domestic drilling site, and the porosity of the sample is tested by using a nuclear magnetic resonance-density balance method, and the test results are shown in Table 2.
Because the method is a block sample, the total volume precision measured by a density balance method is higher, the absolute error and the relative error of the measured porosity by the method are calculated by taking the porosity measured by a nuclear magnetic resonance-density balance method as a reference, as shown in a table 2, and the relative error of the measured porosity of the method provided by the invention is less than or equal to 5 percent, and the test precision meets the application test requirements of industries.
Table 2 results of porosity test of sidewall coring core samples
Example 3
In the XX well of the domestic drilling site, the pore volume and the skeleton volume of the drilling cuttings sample are tested by using the method provided by the invention, and the porosity is calculated. Meanwhile, the porosity of the above sample was tested by a conventional drying method and compared with the porosity tested by the method provided by the present invention, and the test results are shown in table 3.
The porosity of the method is found to be larger than that of the traditional drying method by comparing the porosity of the traditional drying method with the porosity of the method. The method is characterized in that the drilling site reservoir fluid localization measurement result is consulted, the test sample layer section is an oil-containing reservoir and is medium-viscosity crude oil, crude oil in the rock debris pore fluid cannot be dried out by drying at 120 ℃ adopted in the site, so that the dry weight of a drying method is larger, calculated porosity is smaller than an actual value, the effect of measuring the rock debris porosity value is larger, the physical property of a measured sample is met, and the effectiveness and the accuracy of the method are verified.
Table 3 results of porosity test for drill cuttings samples
In the description of the present specification, a description referring to terms "one embodiment," "some embodiments," "examples," "specific examples," or "some examples," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiments or examples. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
Furthermore, the terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include at least one such feature. In the description of the present invention, the meaning of "plurality" means at least two, for example, two, three, etc., unless specifically defined otherwise.
While embodiments of the present invention have been shown and described above, it will be understood that the above embodiments are illustrative and not to be construed as limiting the invention, and that variations, modifications, alternatives and variations may be made to the above embodiments by one of ordinary skill in the art within the scope of the invention.
Claims (10)
1. A method for testing the porosity of an irregularly shaped core, the method comprising:
placing a volume scale sample into a sample tube and not exceeding a first mark line of the sample tube, testing to obtain a nuclear magnetic resonance signal S H1 of the volume scale sample, and calculating to obtain a scale coefficient K H,KH=VH/SH1,VH of the volume scale sample as the volume of hydrogen-containing liquid of the volume scale sample, wherein a region between the first mark line of the sample tube and the bottom of the sample tube corresponds to a nuclear magnetic resonance signal linear region;
Taking out the volume scale standard sample, adding the hydrogen-containing liquid into the sample tube until the liquid adding height is between a second mark line and a third mark line of the sample tube, and testing to obtain a nuclear magnetic resonance signal S Hmax of the hydrogen-containing liquid, wherein the region between the first mark line and the second mark line corresponds to a nuclear magnetic resonance signal nonlinear region, and the region between the second mark line and the third mark line corresponds to a highest nuclear magnetic resonance signal region;
Pretreating a sample to be detected, placing the pretreated sample to be detected into a sample tube and not exceeding a first marking line of the sample tube, testing to obtain a nuclear magnetic resonance signal S H2 of the sample to be detected, and calculating to obtain the pore volume V por,Vpor=KH×SH2 of the sample to be detected;
Adding the hydrogen-containing liquid into the sample tube in which the sample to be detected is placed until the liquid adding height is between the second mark line and the third mark line of the sample tube, testing to obtain nuclear magnetic resonance signals S H3 of the sample to be detected and the hydrogen-containing liquid, and calculating to obtain skeleton volume V G,VG=KH×(SHmax-SH3 of the sample to be detected;
Calculating to obtain the porosity of the sample to be measured ，
。
2. The method for testing the porosity of the irregularly shaped core according to claim 1, wherein the method for obtaining the second marker line comprises:
And taking out the volume scale standard sample, continuously adding the hydrogen-containing liquid into the sample tube until the nuclear magnetic resonance signal of the hydrogen-containing liquid is maximum, wherein the liquid level surface corresponding to the maximum nuclear magnetic resonance signal of the hydrogen-containing liquid is the second mark line.
3. The method for testing the porosity of the irregularly shaped core according to claim 1, wherein the pre-treating the sample to be tested comprises: and removing the fluid on the surface of the sample to be detected.
4. The method of claim 1, wherein the nuclear magnetic resonance signal is acquired using a CPMG sequence.
5. The method for testing the porosity of the irregularly shaped core according to claim 1, wherein the hydrogen-containing liquid is a copper sulfate solution with a mass concentration of 1000-1500 ppm.
6. The method for testing the porosity of the irregularly shaped core according to claim 1, wherein adding the hydrogen-containing liquid to the sample tube into which the sample to be tested is placed until a filling height is between the second mark line and the third mark line of the sample tube comprises:
And eliminating bubbles adsorbed on the surface of the sample to be detected.
7. An apparatus for the method of porosity testing of the irregularly shaped core of any one of claims 1 to 6, comprising: the device comprises a magnet unit, a radio frequency unit, a spectrometer unit, a calculation unit and a sample tube;
The magnet unit comprises a magnet which is used for providing a magnetic field for the volume scale standard sample, the hydrogen-containing liquid and the sample to be tested, and the magnetic field strength of the magnet is 0.1-0.2T;
The radio frequency unit is used for detecting nuclear magnetic resonance signals of the volume calibration standard sample, the hydrogen-containing liquid and the sample to be detected, the radio frequency unit comprises a radio frequency coil, the radio frequency coil is an H radio frequency coil with low filling sensitivity, the radio frequency coil is provided with a nuclear magnetic resonance signal linear region, a nuclear magnetic resonance signal nonlinear region and a highest nuclear magnetic resonance signal region, when the liquid level surface of the hydrogen-containing liquid is in the nuclear magnetic resonance signal linear region, the nuclear magnetic resonance signals of the hydrogen-containing liquid are in direct proportion to the volume of the hydrogen-containing liquid, when the liquid level surface of the hydrogen-containing liquid is in the nuclear magnetic resonance signal nonlinear region, the nuclear magnetic resonance signals of the hydrogen-containing liquid and the volume of the hydrogen-containing liquid are in a nonlinear monotonically increasing rule, when the liquid level surface of the hydrogen-containing liquid is in the highest nuclear magnetic resonance signal region, the nuclear magnetic resonance signals of the hydrogen-containing liquid reach the maximum value, and the nuclear magnetic resonance signal deviation of the hydrogen-containing liquid in the highest nuclear magnetic resonance signal region is less than or equal to +/-1%;
The spectrometer unit is used for controlling the radio frequency unit to collect nuclear magnetic resonance signals of the volume scale standard sample, the hydrogen-containing liquid and the sample to be detected;
the computing unit is used for computing the porosity of the sample to be tested;
The sample tube is used for placing the volume scale standard sample, the hydrogen-containing liquid and the sample to be measured in the radio frequency coil, a first mark line, a second mark line and a third mark line are arranged on the surface of the sample tube, the region between the first mark line and the bottom of the sample tube corresponds to the nuclear magnetic resonance signal linear region, the region between the first mark line and the second mark line corresponds to the nuclear magnetic resonance signal nonlinear region, and the region between the second mark line and the third mark line corresponds to the highest nuclear magnetic resonance signal region.
8. The apparatus of the porosity testing method for irregularly shaped cores of claim 7, wherein the radio frequency coil has an inductance range of。
9. The device of the porosity testing method for the irregularly-shaped core according to claim 7, wherein the sample tube comprises a main body and a sealing cover, the main body is of a cylinder structure with one end open, the main body and the sealing cover form an accommodating space, the accommodating space is used for accommodating the volume scale standard sample, the hydrogen-containing liquid and the sample to be tested, an internal thread is arranged at the opening of the main body, an external thread matched with the internal thread is arranged on the sealing cover, and the sealing cover can move along a preset direction through the internal thread to seal the main body.
10. The apparatus of the porosity testing method for irregularly shaped cores according to claim 9, wherein the surface of the sealing cover is provided with knurling, and the end of the main body away from the opening is arc-shaped.
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